CN112745661B - Material with high dielectric constant under high-frequency electric field and suitable for reflow soldering and LDS (laser direct structuring) and preparation method thereof - Google Patents
Material with high dielectric constant under high-frequency electric field and suitable for reflow soldering and LDS (laser direct structuring) and preparation method thereof Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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Abstract
The application discloses a material with a high dielectric constant under a high-frequency electric field and suitable for reflow soldering and LDS (laser direct structuring) and a preparation method thereof, relates to the technical field of high polymer materials, and aims to solve the problem that the reflow soldering and LDS (Laser Direct Structuring laser direct structuring technology) cannot be simultaneously met due to the fact that the thermal deformation temperature of the material with the high dielectric constant does not meet the requirements. The technical scheme is characterized by comprising, by mass, 20-40% of high-temperature nylon, 10-20% of glass fiber, 30-50% of ceramic powder and 8-15% of pigment; the dielectric constant of the material is 4-10 under the high-frequency electric field of 2-20GHz, and the thermal deformation temperature is more than 260 ℃. When high-temperature nylon is used as matrix resin, for example, 2.0GHz,6.0GHz and 10.1GHz are taken, dielectric constant values are all in the range of 4-10, the thermal deformation temperature is more than 260 ℃, and the reflow soldering and LDS (Laser Direct Structuring laser direct molding technology) are satisfied.
Description
Technical Field
The application relates to the technical field of high polymer materials, in particular to a material which has high dielectric constant under a high-frequency electric field and is suitable for reflow soldering and LDS (laser direct structuring) and a preparation method thereof.
Background
For the dielectric constant of communication materials, research is focused mainly on the low frequency phase, and rarely involves the use of high frequency electric fields. In recent years, as a new generation of communication fields develop, in some devices related to the fields, dielectric properties of materials, particularly dielectric properties under high-frequency electric fields, are increasingly required because of high-frequency electric fields and signal transmission.
The preparation of polymer composites is an effective way to increase the dielectric constant. The dielectric constant can be improved by filling high dielectric constant ceramic powder into the polymer matrix, and ceramic fillers reported in literature are barium titanate, copper calcium titanate, titanium dioxide, silicon dioxide, lead zincate, lead magnesium aluminate and the like. Another approach is to fill conductive materials, such as carbon materials like graphite, carbon black, graphene, carbon nanotubes, etc., and metallic materials like silver particles, aluminum particles, liquid metals, etc., into the polymer matrix.
At present, some materials with high dielectric constants cannot meet the requirements of reflow soldering and LDS (Laser Direct Structuring laser direct structuring technology, LDS for short) at the same time because the thermal deformation temperature does not meet the requirements, so that further improvement is needed.
Disclosure of Invention
One of the purposes of the present application is to provide a material suitable for high-frequency electric field, reflow soldering and LDS, which has the effects of realizing high dielectric constant under high-frequency electric field and realizing reflow soldering and LDS.
The technical aim of the application is realized by the following technical scheme:
the material with high dielectric constant under high-frequency electric field and suitable for reflow soldering and LDS comprises the following components in percentage by mass,
the dielectric constant of the material is 4-10 under the high-frequency electric field of 2-20GHz, and the thermal deformation temperature is more than 260 ℃.
The application is further provided with: the high-temperature nylon is one of PA4T, PA6T, PA T, PA10T, PA.
The application is further provided with: the dielectric constant of the high-temperature nylon is 4.3, the melting point of the high-temperature nylon is 290-320 ℃, and the density of the high-temperature nylon is 1.12-1.16g/cm 3 。
The application is further provided with: the dielectric constant of the glass fiber is 4.5-5.0, and the density of the glass fiber is 2.54g/cm 3 。
The application is further arranged to: the ceramic powder is a mixture of titanium dioxide and aluminum oxide and has a density of 4.0g/cm 3 。
The application also aims to provide a preparation method of the material which has high dielectric constant under a high-frequency electric field and is suitable for reflow soldering and LDS.
In order to achieve the above purpose, the present application provides the following technical solutions: comprises the following steps of the method,
step1 weighing: weighing high-temperature nylon, glass fiber, ceramic powder and pigment according to the proportion;
step2 premixing: adding high-temperature nylon, ceramic powder and pigment into a mixer, and uniformly premixing;
step3 extrusion: adding the mixture obtained by premixing into a main hopper of a double-screw extruder, adding glass fibers into a side feeding hopper of the double-screw extruder, and extruding through the double-screw extruder;
step4, cooling: immersing the molten mixture obtained by extrusion in a water tank;
step5 granulating: adding the cooled product into a granulator, dragging and granulating by using the granulator, and continuously granulating;
step6, screening: adding the product obtained by granulation into a sieving machine, and uniformly treating the particles by a vibrating sieve;
step7, drying: drying the product obtained by screening;
step8, spline preparation: after the particles are cooled, the particles are added into an injection molding machine, the preparation of test bars is carried out by the injection molding machine and setting reasonable technological parameters, and the test bars can be tested after cooling.
The application is further provided with: in Step3, the extrusion temperature of the twin-screw extruder is set to 300-330 ℃, and the rotation speed of the host machine is 300rpm.
The application is further provided with: in Step8, the injection pressure of the injection molding machine is 69-103MPa, the mold temperature is 100-135 ℃, and the melting temperature is 300-330 ℃.
The application is further provided with: step7, drying at 100-130deg.C for 4-6 hr.
In summary, the beneficial technical effects of the application are as follows:
when high-temperature nylon is used as matrix resin, the dielectric constant values are in the range of 4-10, the thermal deformation temperature is more than 260 ℃ and the reflow soldering and LDS are satisfied by taking 2.0GHz,6.0GHz and 10.1GHz as examples.
Detailed Description
The following detailed description of the preferred embodiments of the application is provided to enable those skilled in the art to more readily understand the advantages and features of the application and to make a clear and concise definition of the scope of the application.
It is worth noting that the high temperature nylon used in the application is one of PA4T, PA, T, PA, 9, T, PA, 10 and T, PA, the dielectric constant of the high temperature nylon is 4.3, the melting point of the high temperature nylon is 290-320 ℃, and the density of the high temperature nylon is 1.12-1.16g/cm 3 ；
The dielectric constant of the glass fiber is 4.5-5.0, and the density of the glass fiber is 2.54g/cm 3 ；
The ceramic powder is titanium dioxide and alumina mixture and has a density of 4.0g/cm 3 ；
The pigment is copper complex pigment;
polyphenylene Sulfide (PPS) has a dielectric constant of 3-3.3, a melting point of 270-290 ℃ and a density of 1.3-1.4g/cm 3 ；
The dielectric constant of the Liquid Crystal Polymer (LCP) is 3.3, the melting point is 350-360 ℃ and the density is 1.41g/cm 3 ；
The other raw materials are all common commercial products, so the sources thereof are not particularly limited.
Examples 1 to 2
According to the mass ratio, the contents of the components of the material which has high dielectric constant under the high-frequency electric field and is suitable for reflow soldering and LDS are shown in the following table:
TABLE 1 content of the components of the materials having a high dielectric constant and suitable for reflow soldering and LDS in examples 1-2 under a high frequency electric field
| Component (A) | Example 1 | Example 2 |
| High temperature nylon | 35kg | 33kg |
| Glass fiber | 10kg | 10kg |
| Ceramic powder | 40kg | 46kg |
| Pigment | 15kg | 11kg |
Comparative examples 1 to 2
The contents of various components of the PPS modified material and the LCP modified material according to the mass ratio are shown in the following table:
TABLE 2 content of the components of PPS-modified material and LCP-modified material in comparative examples 1-2
| Component (A) | Comparative example 1 | Comparative example 2 |
| PPS | 41kg | / |
| LCP | / | 35kg |
| Glass fiber | 10kg | 10kg |
| Calcium carbonate | 10kg | / |
| Ceramic powder | 25kg | 40kg |
| Pigment | 10kg | 15kg |
| Toughening agent | 4kg | / |
Example 3
Based on example 1, the preparation of example 1 is as follows,
step1 weighing: weighing 35kg of high-temperature nylon (PA 10T), 10kg of glass fiber, 40kg of ceramic powder and 15kg of pigment according to the proportion;
step2 premixing: adding high-temperature nylon, ceramic powder and pigment into a mixer, and uniformly premixing;
step3 extrusion: adding the mixture obtained by premixing into a main hopper of a double-screw extruder, adding glass fibers into a side feeding hopper of the double-screw extruder, and extruding through the double-screw extruder; the extrusion temperature is set to 300-330 ℃, and the rotation speed of a host machine is 300rpm;
step4, cooling: immersing the molten mixture obtained by extrusion in a water tank;
step5 granulating: adding the cooled product into a granulator, dragging and granulating by using the granulator, and continuously granulating;
step6, screening: adding the product obtained by granulation into a sieving machine, and uniformly treating the particles by a vibrating sieve;
step7, drying: drying the sieved product at 100-130 ℃ for 4-6h;
step8, spline preparation: after the particles are cooled, the particles are added into an injection molding machine, the injection molding pressure of the injection molding machine is set to 69MPa, the mold temperature is set to 110 ℃, the melting temperature is set to 300-330 ℃, the preparation of test bars is carried out, and the test bars can be tested after cooling.
Example 4
Based on example 2, the preparation of example 2 is as follows,
step1 weighing: weighing 33kg of high-temperature nylon (PA 10T), 10kg of glass fiber, 46kg of ceramic powder and 11kg of pigment according to the proportion;
step2 premixing: adding high-temperature nylon, ceramic powder and pigment into a mixer, and uniformly premixing;
step3 extrusion: adding the mixture obtained by premixing into a main hopper of a double-screw extruder, adding glass fibers into a side feeding hopper of the double-screw extruder, and extruding through the double-screw extruder; the extrusion temperature was set at 330℃and the host rotation speed at 300rpm;
step4, cooling: immersing the molten mixture obtained by extrusion in a water tank;
step5 granulating: adding the cooled product into a granulator, dragging and granulating by using the granulator, and continuously granulating;
step6, screening: adding the product obtained by granulation into a sieving machine, and uniformly treating the particles by a vibrating sieve;
step7, drying: drying the sieved product at 100-130 ℃ for 4-6h;
step8, spline preparation: after the particles are cooled, the particles are added into an injection molding machine, the injection molding pressure of the injection molding machine is set to be 103MPa, the mold temperature is set to be 110 ℃, the melting temperature is set to be 300-330 ℃, the preparation of test bars is carried out, and the test bars can be tested after cooling.
Comparative example 3
The matrix resin was replaced with polyphenylene sulfide (PPS) from high temperature nylon.
Based on comparative example 1, comparative example 1 was prepared as follows,
step1 weighing: 41kg of polyphenylene sulfide (PPS), 10kg of glass fiber, 10kg of calcium carbonate, 25kg of ceramic powder, 10kg of pigment and 4kg of toughening agent are weighed according to the proportion;
step2 premixing: adding polyphenylene sulfide, glass fiber, calcium carbonate, ceramic powder and pigment into a mixer, and uniformly premixing;
step3 extrusion: adding the mixture obtained by premixing into a main hopper of a double-screw extruder, adding glass fibers into a side feeding hopper of the double-screw extruder, and extruding through the double-screw extruder; the extrusion temperature was set at 310℃and the host rotation speed was 300rpm;
step4, cooling: immersing the molten mixture obtained by extrusion in a water tank;
step5 granulating: adding the cooled product into a granulator, dragging and granulating by using the granulator, and continuously granulating;
step6, screening: adding the product obtained by granulation into a sieving machine, and uniformly treating the particles by a vibrating sieve;
step7, drying: drying the product obtained by screening at 150 ℃ for 4-6 hours;
step8, spline preparation: after the particles are cooled, the particles are added into an injection molding machine, the injection molding pressure of the injection molding machine is set to 69MPa, the mold temperature is 130 ℃, the melting temperature is 300-330 ℃, the preparation of test bars is carried out, and the test bars can be tested after cooling.
Comparative example 4
The matrix resin is replaced by Liquid Crystal Polymer (LCP) from high temperature nylon.
Based on comparative example 2, comparative example 2 was prepared as follows,
step1 weighing: weighing 35kg of Liquid Crystal Polymer (LCP), 10kg of glass fiber, 40kg of ceramic powder and 15kg of pigment according to the proportion;
step2 premixing: adding liquid crystal polymer, ceramic powder and pigment into a mixer, and uniformly premixing;
step3 extrusion: adding the mixture obtained by premixing into a main hopper of a double-screw extruder, adding glass fibers into a side feeding hopper of the double-screw extruder, and extruding through the double-screw extruder; the extrusion temperature was set at 330℃and the host rotation speed at 300rpm;
step4, cooling: immersing the molten mixture obtained by extrusion in a water tank;
step5 granulating: adding the cooled product into a granulator, dragging and granulating by using the granulator, and continuously granulating;
step6, screening: adding the product obtained by granulation into a sieving machine, and uniformly treating the particles by a vibrating sieve;
step7, drying: drying the product obtained by screening at 150 ℃ for 4-6 hours;
step8, spline preparation: after the particles are cooled, the particles are added into an injection molding machine, the injection molding pressure of the injection molding machine is set to be 103MPa, the temperature of a mold is set to be 135 ℃, the melting temperature is set to be 320-370 ℃, the preparation of test bars is carried out, and the test bars can be tested after cooling.
The materials prepared in examples 3-4 and comparative examples 3-4 were subjected to related performance tests, which were respectively American Society for Testing and Materials (ASTM):
the material was tested for dielectric constant at frequencies of 2.0ghz,6.0ghz,10.1ghz according to astm d 150;
tensile strength was tested according to astm d 638;
flexural strength and flexural modulus were tested according to astm d 790;
impact properties were tested according to astm d256 and astm d 4812;
the test results are shown in the following table.
TABLE 3 Performance test results for each of the materials of examples 3-4, comparative examples 3-4
From the above table, when polyphenylene sulfide (PPS) and Liquid Crystal Polymer (LCP) are used as matrix resins, dielectric constant values are in the range of 4-10 at 2.0GHz,6.0GHz, and 10.1GHz, but the heat distortion temperatures are less than 260 ℃, so that the reflow soldering and the LDS (Laser Direct Structuring laser direct molding technique) cannot be satisfied at the same time;
when high-temperature nylon is used as matrix resin, the dielectric constant values are in the range of 4-10 with the thermal deformation temperature being more than 260 ℃ by taking 2.0GHz,6.0GHz and 10.1GHz as examples, and simultaneously, the reflow soldering and LDS (Laser Direct Structuring laser direct molding technology) are satisfied.
The foregoing description is only illustrative of the present application and is not intended to limit the scope of the application, and all equivalent structures or equivalent processes or direct or indirect application in other related technical fields are included in the scope of the present application.
Claims (7)
1. The material with high dielectric constant under high frequency electric field and suitable for reflow soldering and LDS is characterized in that: comprises the following components in percentage by mass,
PA10T 20~40%
10-20% of glass fiber
30-50% of ceramic powder
8-15% of pigment;
the ceramic powder is a mixture of titanium dioxide and aluminum oxide; the dielectric constant of the material is 4-10 under the high-frequency electric field of 2-20GHz, and the thermal deformation temperature is more than 260 ℃;
the preparation method of the material which has high dielectric constant under the high-frequency electric field and is suitable for reflow soldering and LDS comprises the following steps,
stepl weighing: weighing PA10T, glass fiber, ceramic powder and pigment according to the proportion;
step2 premixing: adding PA10T, ceramic powder and pigment into a mixer, and uniformly premixing;
step3 extrusion: adding the mixture obtained by premixing into a main hopper of a double-screw extruder, adding glass fibers into a side feeding hopper of the double-screw extruder, and extruding through the double-screw extruder;
step4, cooling: immersing the molten mixture obtained by extrusion in a water tank;
step5 granulating: adding the cooled product into a granulator, dragging and granulating by using the granulator, and continuously granulating;
step6, screening: adding the product obtained by granulation into a sieving machine, and uniformly treating the particles by a vibrating sieve;
step7, drying: drying the product obtained by screening;
step8, spline preparation: after the particles are cooled, the particles are added into an injection molding machine, the preparation of test bars is carried out by the injection molding machine and setting reasonable technological parameters, and the test bars can be tested after cooling.
2. The material with high dielectric constant under high frequency electric field according to claim 1 and suitable for reflow soldering, LDS, wherein: the dielectric constant of the glass fiber is 4.5-5.0, and the density of the glass fiber is 2.54g/cm 3 。
3. The material with high dielectric constant under high frequency electric field according to claim 1 and suitable for reflow soldering, LDS, wherein: the ceramic powder is titanium dioxide and alumina mixture with the density of 4.0g/cm 3 。
4. A method for preparing a material having a high dielectric constant in a high frequency electric field and suitable for reflow soldering and LDS as claimed in any one of claims 1 to 3, characterized in that: comprises the following steps of the method,
stepl weighing: weighing PA10T, glass fiber, ceramic powder and pigment according to the proportion;
step2 premixing: adding PA10T, ceramic powder and pigment into a mixer, and uniformly premixing;
step3 extrusion: adding the mixture obtained by premixing into a main hopper of a double-screw extruder, adding glass fibers into a side feeding hopper of the double-screw extruder, and extruding through the double-screw extruder;
step4, cooling: immersing the molten mixture obtained by extrusion in a water tank;
step5 granulating: adding the cooled product into a granulator, dragging and granulating by using the granulator, and continuously granulating;
step6, screening: adding the product obtained by granulation into a sieving machine, and uniformly treating the particles by a vibrating sieve;
step7, drying: drying the product obtained by screening;
step8, preparing sample bars, namely adding the particles into an injection molding machine after cooling the particles, preparing test sample bars by the injection molding machine and setting reasonable technological parameters, and testing after cooling.
5. The method for preparing a material with high dielectric constant under high-frequency electric field and suitable for reflow soldering and LDS according to claim 4, wherein the method comprises the following steps: in Step3, the extrusion temperature of the twin-screw extruder is set to 300-330 ℃, and the rotation speed of the host machine is 300rpm.
6. The method for preparing a material with high dielectric constant under high-frequency electric field and suitable for reflow soldering and LDS according to claim 4, wherein the method comprises the following steps: in Step8, the injection pressure of the injection molding machine is 69-103MPa, the mold temperature is 100-135 ℃, and the melting temperature is 300-330 ℃.
7. The method for preparing a material with high dielectric constant under high-frequency electric field and suitable for reflow soldering and LDS according to claim 4, wherein the method comprises the following steps: step7, drying at 100-130 ℃ for 4-6h.
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| CN102066473A (en) * | 2008-05-23 | 2011-05-18 | 沙伯基础创新塑料知识产权有限公司 | High dielectric constant laser direct structuring materials |
| CN102952388A (en) * | 2012-11-30 | 2013-03-06 | 深圳市博恩实业有限公司 | High dielectric constant thermally conductive plastic and preparation method thereof |
| CN104918991A (en) * | 2012-12-19 | 2015-09-16 | 帝斯曼知识产权资产管理有限公司 | Thermoplastic composition |
| CN106133060A (en) * | 2014-03-25 | 2016-11-16 | 帝斯曼知识产权资产管理有限公司 | Polymer composition, its goods and the method preparing its goods |
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